CN112110442A - Modified graphene oxide and preparation method and application thereof - Google Patents
Modified graphene oxide and preparation method and application thereof Download PDFInfo
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- C09K8/584—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific surfactants
Abstract
The application discloses a modified graphene oxide, and a preparation method and application thereof. And (3) grafting a hydrophobic chain segment on the surface of the graphene oxide sheet layer nano material to ensure that the graphene oxide sheet layer nano material shows higher hydrophobicity. The microemulsion dispersion technology is adopted, and the microemulsion dispersion technology is dispersed in water to form the nano drag-reducing injection-increasing agent similar to microemulsion. The lamellar nano material has stronger rock adsorption force than the spherical polysilicon material, the effect is longer, and the popularization of the subsequent market is more promising.
Description
Technical Field
The application relates to modified graphene oxide and a preparation method and application thereof, and belongs to the technical field of graphene oxide materials.
Background
The low permeability and heavy oil resources account for about 2/3 total petroleum resources, and the development difficulty is large. The conventional anti-drag injection-increasing technology comprises two major types, namely reservoir transformation, wherein the reservoir porosity is changed, the injection fluid resistance is reduced, the water injection amount is increased, and the conventional method for changing the reservoir porosity comprises fracturing and acidification. The disadvantage is irreversible damage to the formation, which is often irreversible; the scale is not well controlled, unidirectional flow is easy to form, and oil reservoir flooding and water channeling are caused; and secondly, the resistance of formation fluid and the rock surface is reduced through rock surface modification, and the resistance-reducing injection-increasing modes mainly comprise a surfactant injection-increasing technology and an organic molecular film resistance-reducing injection-increasing technology. The surfactant has compatibility problem in the process of reducing and increasing injection, secondary precipitation is easy to occur due to incompatibility of the surfactant and oil reservoir fluid, so that the stratum is blocked, the performance of the surfactant is obviously influenced by the temperature of the stratum, and the surfactant is only suitable for reducing and increasing injection of a water injection well with lower oil reservoir temperature.
The pressure reduction and injection increase of the water well are difficult problems before oil field science and technology personnel, and a new injection increase process is necessary. The active nano drag reducer is a hydrophobic material with nano-scale size, can solve the problems of pressure reduction and injection increase in the water injection development process of a low-permeability oil reservoir, has the advantages of simple construction, no environmental pollution, small influence of the oil reservoir temperature and the like, and has great application prospect.
The nanometer drag reducer used in the oil field at present is an active nanometer material taking hydrophobic polysilicon material as a main component, but the hydrophobic polysilicon material has larger discrete particle size and is easy to aggregate and block when entering a stratum from a shaft, the adsorption performance of the polysilicon material on the surface of the stratum rock is poor, the anti-scouring capability to water flow is poor, and the nanometer polysilicon material is easy to migrate along with the extension of the subsequent water flooding time, so that the secondary blocking to an oil reservoir is caused. Therefore, the nano drag reducer which has excellent adsorption performance and small blocking side effect and is suitable for the water injection development of the low-permeability reservoir has great significance.
Disclosure of Invention
According to one aspect of the application, a modified graphene oxide is provided, and a hydrophobic chain segment is grafted on the surface of a graphene oxide sheet-layer nano material, so that the graphene oxide sheet-layer nano material shows high hydrophobicity. The microemulsion dispersion technology is adopted, and the microemulsion dispersion technology is dispersed in water to form the nano drag-reducing injection-increasing agent similar to microemulsion. After the lamella nanometer water-based dispersion liquid is injected into the stratum, phase separation can be carried out under the stratum environment, and the hydrophobic lamella nanometer material is released. The lamellar hydrophobic nano material is adsorbed on the surface of the rock by strong force, so that the thickness of a hydration film on the surface of the rock is reduced or adsorbed water is removed. Meanwhile, after the hydrophobic lamellar nano material is adsorbed on the surface of the rock, the wettability of the rock can be changed from hydrophilicity to neutral wettability or hydrophobicity, the interfacial force between injected water and the rock is reduced, and the water phase permeability is improved, so that the effects of reducing drag and increasing injection are achieved. The lamellar nano material has stronger rock adsorption force than the spherical polysilicon material, the effect is longer, and the popularization of the subsequent market is more promising.
According to a first aspect of the present application, there is provided a modified graphene oxide, wherein the modified graphene oxide is obtained by chemically grafting a siloxane compound and graphene oxide.
Optionally, a functional group on the surface of the graphene oxide and a hydroxyl group on the surface of the siloxane compound are subjected to a chemical reaction to obtain the modified graphene oxide.
Optionally, the siloxane-based compound is selected from silane coupling agents;
preferably, the silane coupling agent is selected from at least one of gamma-methacryloxypropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, and gamma- (2, 3-glycidoxy) propyltrimethoxysilane.
Optionally, the particle size of the modified graphene oxide is 200-300 nm.
Optionally, the viscosity of the modified graphene oxide is 1-2 cP.
According to another aspect of the present application, there is also provided a preparation method of the above modified graphene oxide, the preparation method at least including:
and reacting a mixture containing graphene oxide and siloxane compounds to obtain the modified graphene oxide.
Optionally, the molar ratio of the graphene oxide to the siloxane compound is 5:1-20: 1.
Optionally, the upper limit of the molar ratio of the graphene oxide to the siloxane is independently selected from 20: 1. 15: 1. 10: 1, the lower limit is independently selected from 5: 1. 15: 1. 10: 1.
optionally, the reaction conditions are: the reaction temperature is 50-70 ℃; the reaction time is 8-12 h.
Optionally, the particle size of the graphene oxide is 80-150 nm.
Optionally, the upper limit of the particle size of the graphene oxide is independently selected from 150nm, 120nm and 90nm, and the lower limit is independently selected from 80nm, 120nm and 90 nm.
Optionally, the method comprises at least: and mixing the dispersion liquid containing the graphene oxide and the solution containing the siloxane compound, and reacting to obtain the modified graphene oxide.
Optionally, the dispersion liquid containing graphene oxide comprises a dispersant I; the dispersant I is water.
Preferably, the dispersion liquid containing graphene oxide contains 1000 to 2000ppm of graphene oxide.
Optionally, the siloxane compound-containing solution comprises a solvent I; the solvent I is selected from alcohol compounds.
Preferably, the concentration of the solution containing the siloxane compound is 100-200 ppm.
According to a third aspect of the application, a nano drag reduction and injection enhancement agent is also provided, which comprises a dispersant II, a solvent II and modified graphene oxide;
the modified graphene oxide is at least one selected from the modified graphene oxide and the modified graphene oxide prepared by the method.
Alternatively, solvent II is selected from water.
Optionally, the nano drag reducing and injection enhancing agent comprises: : 0.1 to 0.2 wt% of modified graphene oxide; 2 to 5 wt% of a dispersant II; 94.9 wt% to 97.9 wt%.
Optionally, the dispersant II is selected from a surfactant.
Preferably, the surfactant is selected from at least one of tween-80, tween-20 and Sodium Dodecyl Sulfate (SDS).
According to a fourth aspect of the present application, there is also provided a method for preparing the above-mentioned nano drag-reducing injection-increasing agent, the method at least comprising: and stirring a mixture containing the modified graphene oxide, the dispersant II and the solvent II to obtain the nano anti-drag injection-increasing agent.
Optionally, the method comprises at least: and mixing the modified graphene oxide with a solution containing a dispersant II and a solvent II, stirring, adding the solvent II, and continuously stirring to obtain the nano anti-drag injection-increasing agent.
Optionally, in the solution containing the dispersant II and the solvent II, the mass ratio of the dispersant II to the solvent II is 1: 19-1: 49.
According to the last aspect of the application, the application of at least one of the nano drag-reducing injection-increasing agent and the nano drag-reducing injection-increasing agent prepared by the method in low permeability oil fields is also provided.
The beneficial effects that this application can produce include:
according to the invention, the lamellar graphene oxide with stronger rock adsorbability is used as a modified base material, and the modified base material is subjected to hydrophobic modification and dispersing agent dispersion to form the water-based carbon nanofluid, so that the water-based carbon nanofluid has stronger time for depressurization and injection increase under the stratum compared with spherical silicon dioxide nanofluid, and has better popularization and application prospects.
Drawings
FIG. 1 is a graph of the particle size distribution of Nanometric drag reducer A;
fig. 2 is a graph of a temperature and salt tolerance test sample of the nano drag reducer a.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
The raw materials in the examples of the present application were all purchased commercially, unless otherwise specified.
The nano drag reducer in the embodiment of the application is the nano drag reduction and injection enhancement agent in the application.
Graphene oxide in the examples of the present application was purchased from senary element corporation, changzhou, model SE 3122.
The temperature-resistant and salt-tolerant test in the embodiment of the application adopts a Shanghai constant BPG-9070A constant-temperature oven;
particle size testing was performed using a malvern Nano ZSE in england.
Possible embodiments are described below:
the invention provides a novel preparation method of a drag reducer. The method comprises the following specific steps:
and (1) putting a certain amount of graphene oxide water-based dispersion liquid with the concentration of 5mg/mL into a 500mL three-neck flask, and putting the three-neck flask into a water bath kettle at 60 ℃ for heating.
Step (2) respectively preparing the following graphene oxide according to a certain mass ratio: weighing a certain mass of siloxane compound, heating and dissolving the siloxane compound in absolute ethyl alcohol.
Step (3) adding the fully dissolved absolute ethanol solution of the siloxane compound into a three-neck flask added with the graphene oxide dispersion liquid within a certain time; the mixed solution is heated in a water bath at 60 ℃, stirred and refluxed for a certain time, and is centrifuged or dried after the reaction is finished;
weighing a certain mass of dispersant, adding deionized water, and fully stirring for a certain time;
weighing a certain amount of the hydrophobic modified graphene oxide obtained in the step (3), slowly adding the hydrophobic modified graphene oxide into the mixed solution, and rapidly stirring while adding until the hydrophobic graphene oxide is completely dispersed;
slowly adding the emulsion into a 200mL beaker filled with deionized water with a certain mass, stirring at a high speed while adding, and then carrying out water bath and ultrasonic treatment for a certain time to form a uniform black solution;
step (7) carrying out particle size test on the water-based graphene oxide fluid uniformly dispersed in the step (6), and carrying out temperature and salt resistance test, wherein the particle size distribution is relatively uniform, and the water-based graphene oxide fluid has good temperature and salt resistance;
step (8) absorbing the water-based graphene oxide fluid uniformly dispersed in the step (6) on the wall of the Ubbelohde viscometer, testing the time of deionized water flowing through the Ubbelohde viscometer before and after absorption, and taking the average value of three measurements;
the relevant content in the technical scheme of the preparation method is explained as follows:
1. the content of the graphene oxide in the step (1) is 100-200mL, and the particle size is 80-150 nm;
2. the ratio of the graphene oxide to the siloxane compound in the step (2) is 5:1-20:1, wherein the siloxane compound is a silane coupling agent, and the content of ethanol is 200-400 mL;
3. the adding time in the step (3) is 10-30min, and the reaction time is 8-12 h;
4. the mass ratio of the dispersing agent to the hydrophobically modified graphene oxide in the step (4) is 50:1-20:1, the type of the dispersing agent is surfactant, and the content of deionized water is 10-20 mL;
5. in the step (5), the content of the hydrophobically modified graphene oxide is 200 mg-;
6. the content of the deionized water in the step (6) is 80-90 mL;
7. in the step (7), the particle size of the water-based graphene oxide fluid is 200-300nm, and the particle size is 3w NaCl +1200CaCl at 70 DEG C2Under the mineralization degree, no precipitate is generated, the particle size is basically not changed, and the composite material has temperature resistance and salt tolerance;
8. in the step (8), after the hydrophobic modified water-based graphene oxide fluid is adsorbed, the time of deionized water flowing through an Ubbelohde viscometer can be reduced by 0.87-1.50s, and the hydrophobic modified graphene oxide is proved to have a certain drag reduction effect.
Example 1
Step (1), 100mL of 5mg/mL graphene oxide (particle size of 150nm) water-based dispersion liquid is placed in a 1L three-neck flask, and the three-neck flask is placed in a 60 ℃ water bath and heated.
Step (2) 0.1g of a siloxane compound γ -methacryloxypropyltrimethoxysilane (500ppm) (graphene oxide GO: siloxane compound mass ratio: 5: 1) was weighed and dissolved in 400mL of anhydrous ethanol under heating.
Step (3) adding the fully dissolved absolute ethanol solution of the siloxane compound into the three-neck flask of the graphene oxide dispersion liquid within 20 min; and (3) heating the mixed solution in a water bath at 60 ℃, stirring and refluxing for 10 hours, and after the reaction is finished, drying to obtain the modified graphene oxide No. 1.
Example 2
Step (1) 100mL of a graphene oxide water-based dispersion solution (particle size 100nm) with a concentration of 5mg/mL was placed in a 1L three-necked flask, and the three-necked flask was heated in a 50 ℃ water bath.
Step (2), 0.025g of siloxane compound gamma-aminopropyltriethoxysilane (200ppm) (graphene oxide GO: siloxane compound mass ratio of 20: 1) was weighed and dissolved in 400mL of absolute ethanol under heating.
Step (3) adding the fully dissolved absolute ethanol solution of the siloxane compound into the three-neck flask of the graphene oxide dispersion liquid within 10 min; and (4) heating the mixed solution in a water bath at 50 ℃, stirring and refluxing for 8 hours, and after the reaction is finished, drying to obtain the modified graphene oxide 2 #.
Example 3
Step (1) 200mL of a 5mg/mL graphene oxide water-based dispersion (particle size of 80nm) was placed in a 1L three-necked flask, and the three-necked flask was heated in a 70 ℃ water bath.
Step (2) 0.2g of siloxane compound γ - (2, 3-glycidoxy) propyltrimethoxysilane (400ppm) (graphene oxide GO: siloxane compound mass ratio: 5: 1) was weighed and dissolved in 300mL of absolute ethanol under heating.
Step (3) adding the fully dissolved absolute ethanol solution of the siloxane compound into the three-neck flask of the graphene oxide dispersion liquid within 30 min; and (3) heating the mixed solution in a water bath at 70 ℃, stirring and refluxing for 12h, and drying after the reaction is finished to obtain the modified graphene oxide 3 #.
Example 4
Weighing 2g of dispersant Tween-80, adding 10g of deionized water, and stirring for 30 min;
weighing 0.1g of hydrophobic modified graphene oxide No. 1, slowly adding the hydrophobic modified graphene oxide No. 1 into the mixed solution, and rapidly stirring while adding until the hydrophobic graphene oxide is completely dispersed;
slowly adding the uniform emulsion into a 200mL beaker filled with 87.9g of deionized water, stirring at high speed while adding, and then carrying out water bath ultrasonic treatment for 2 hours to form a uniform black solution, namely the nano anti-drag injection-increasing agent A.
Example 5
Weighing 3.5g of dispersant Tween-80, adding 15g of deionized water, and stirring for 30 min;
weighing 0.15g of hydrophobic modified graphene oxide No. 2, slowly adding the hydrophobic modified graphene oxide No. 2 into the mixed solution, and rapidly stirring while adding until the hydrophobic graphene oxide is completely dispersed;
slowly adding the uniform emulsion into a 200mL beaker filled with 81.35g of deionized water, stirring at high speed while adding, and then carrying out water bath ultrasonic treatment for 2 hours to form a uniform black solution, namely the nano anti-drag injection-increasing agent B.
Example 6
Weighing 5g of dispersant Tween-80, adding 20g of deionized water, and stirring for 30 min;
weighing 0.1g of hydrophobic modified graphene oxide No. 3, slowly adding the hydrophobic modified graphene oxide No. 3 into the mixed solution, and rapidly stirring while adding until the hydrophobic graphene oxide is completely dispersed;
slowly adding the uniform emulsion into a 200mL beaker filled with 74.9g of deionized water, stirring at high speed while adding, and then carrying out water bath and ultrasonic treatment for 2 hours to form a uniform black solution, namely the nano anti-drag injection-increasing agent C.
Example 7 particle size testing
The Nano drag reducer prepared in examples 4 to 6 is diluted to 100ppm with deionized water, and put into a marwen Zetasizer Nano ZSE sample tank, and a click test is performed, three times of each sample are measured, and an average value is taken, taking the Nano drag reducer a in example 4 as a representative, and as shown in fig. 1, a particle size distribution diagram of the Nano drag reducer a is shown, and it can be seen that the average particle size of the modified graphene oxide in the Nano drag reducer is 210 nm.
Example 8 temperature and salt resistance stability test
The nano drag reducer prepared in examples 4 to 6 was diluted with simulated brine (3w NaCl +1200 CaCl)2) Diluting to 100ppm, placing in an oven at 70 ℃ for 7d, and observing the stability, wherein the nano drag reducer A is taken as a typical representative, and FIG. 2 is a temperature and salt resistance test sample diagram of the nano drag reducer A, and as can be seen, no particles can be seen with naked eyes.
Example 9 drag reduction effectiveness test
The method comprises the steps of placing the Ubbelohde viscometer in a constant-temperature water bath at 30 ℃, respectively testing the time of deionized water flowing through the Ubbelohde viscometer before and after the nano drag reducer (100ppm) prepared in the examples 4 to 6 is adsorbed (adsorbed for 72 hours) on the wall of the Ubbelohde viscometer, taking the average value of three measurements, taking the nano drag reducer A as a typical representative, and taking the table 1 as the time of the deionized water flowing through the Ubbelohde viscometer before and after the nano drag reducer is adsorbed, wherein the time of the deionized water flowing through the Ubbelohde viscometer is 72.98s from 74.47s after the nano drag reducer is adsorbed, and is reduced by 1.49s, so that the nano drag reducer has a.
TABLE 1
| Nano drag reducer A | First time/s | Second time/s | Third time/s | Average/s |
| Before adsorption | 74.46 | 74.48 | 74.46 | 74.47 |
| After adsorption | 73.06 | 72.95 | 72.94 | 72.98 |
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. The modified graphene oxide is characterized in that the modified graphene oxide is obtained by chemically grafting siloxane compounds and graphene oxide.
2. The modified graphene oxide according to claim 1, wherein the siloxane-based compound is selected from silane coupling agents;
preferably, the silane coupling agent is at least one selected from the group consisting of gamma-methacryloxypropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, and gamma- (2, 3-glycidoxy) propyltrimethoxysilane.
3. The modified graphene oxide according to claim 1, wherein the particle size of the modified graphene oxide is 200-300 nm;
preferably, the viscosity of the modified graphene oxide is 1-2 cP.
4. The method for producing a modified graphene oxide according to any one of claims 1 to 3, characterized by comprising at least:
and reacting a mixture containing graphene oxide and siloxane compounds to obtain the modified graphene oxide.
5. The preparation method according to claim 4, wherein the molar ratio of the graphene oxide to the siloxane compound is 5:1-20: 1;
preferably, the reaction conditions are: the reaction temperature is 50-70 ℃; the reaction time is 8-12 h;
preferably, the particle size of the graphene oxide is 80-150 nm;
preferably, the method comprises at least: mixing the dispersion liquid containing the graphene oxide with the solution containing the siloxane compound, and reacting to obtain the modified graphene oxide;
preferably, the dispersion liquid containing graphene oxide comprises a dispersant I; the dispersant I is water;
preferably, in the dispersion liquid containing the graphene oxide, the content of the graphene oxide is 1000-2000 ppm;
preferably, the solution containing the siloxane compound comprises a solvent I; the solvent I is selected from alcohol compounds;
preferably, the concentration of the solution containing the siloxane compound is 100-200 ppm.
6. The nano anti-drag injection-increasing agent is characterized by comprising a dispersant II, a solvent II and modified graphene oxide;
the modified graphene oxide is at least one selected from the modified graphene oxide of any one of claims 1 to 3 and the modified graphene oxide prepared by the method of claim 4 or 5.
7. The nano drag reducing and injection enhancing agent of claim 6 wherein the solvent II is selected from the group consisting of water;
preferably, the nano drag reduction and injection enhancement agent comprises: 0.1 to 0.2 wt% of modified graphene oxide; 2 to 5 wt% of a dispersant II; 94.9 to 97.9 wt% of solvent II;
preferably, the dispersant II is selected from surfactants;
preferably, the surfactant is selected from at least one of tween-80, tween-20 and sodium dodecyl sulfate.
8. The method for preparing the nano drag-reducing injection-increasing agent as claimed in claim 6 or 7, wherein the method at least comprises: and stirring a mixture containing the modified graphene oxide, the dispersant II and the solvent II to obtain the nano anti-drag injection-increasing agent.
9. The method for preparing according to claim 8, characterized in that it comprises at least:
mixing the modified graphene oxide with a solution containing a dispersant II and a solvent II, stirring, adding the solvent II, and continuously stirring to obtain the nano anti-drag injection-increasing agent;
preferably, in the solution containing the dispersant II and the solvent II, the mass ratio of the dispersant II to the solvent II is 1: 19-1: 49.
10. Use of at least one of the nano drag-reducing and injection-increasing agent of claim 6 or 7, the nano drag-reducing and injection-increasing agent prepared by the method of claim 8 or 9 in low permeability oil fields.
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| CN115895634B (en) * | 2022-11-11 | 2024-01-23 | 长江大学 | Thick oil viscosity reducer composition and preparation method thereof |
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